CN109399611A - A kind of preparation method of carbon nanotube - Google Patents
A kind of preparation method of carbon nanotube Download PDFInfo
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- CN109399611A CN109399611A CN201710699582.0A CN201710699582A CN109399611A CN 109399611 A CN109399611 A CN 109399611A CN 201710699582 A CN201710699582 A CN 201710699582A CN 109399611 A CN109399611 A CN 109399611A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/88—Molybdenum
- B01J23/882—Molybdenum and cobalt
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The invention belongs to synthesizing carbon nanotubes field of material technology.The present invention provides using polyolefin as carbon source, a kind of load type double-metal Co-Mo is catalyst, and carbon black is cracking synergist, then method that physical blending cracks preparation carbon nanotube.It is characterized in that polyolefin is the polyolefin of pure and mild recycling, carbon black is that nanoscale may participate in the synergist of carbon nanotube synthesis and catalyst is bimetallic effective catalyst.Above-mentioned material is blended by definite composition, is carbon nanotube by Pintsch process under high-temp combustion or inert gas shielding.Present device is simple, easy to operate, reproducible, and cost is relatively low, yield is higher, and carbon nanotube mass is good.Belong to resource reutilization using recycling polyolefin and solve environmental pollution, reduces non-carbon impurity in product using nanoscale carbon black, bimetallic catalyst improves carbon nanotube mass.
Description
Technical field
The invention belongs to a kind of technical fields of synthesizing carbon nanotubes material.Disclose one kind using polyolefin as carbon source, with
Load type double-metal Co-Mo is catalyst, is cracking synergist, the new side of concerted catalysis cracking preparation carbon nanotube with carbon black
Method.
Background technique
Carbon nanotube (CNTs) is found so far under high resolution TEM by Electronic Speculum scholar since 1991.Carbon nanotube
It is a kind of novel carbon structure, is the nano crystals of graphite, can abstractively regards as in being surrounded by the graphite flake of hexagon
Mandrel hollow tubular structure made of spiral at a particular angle, sealing two ends.The diameter of carbon nanotube is generally no greater than
100nm, length is then up to micron order, therefore its draw ratio is very big, can be regarded as One-dimensional Quantum material.It is unique close with its
Like one-dimensional cannulated structure, the properties such as special mechanics, calorifics, electromagnetism and exclusive in each field potentially make
With value, quickly the research emphasis as subjects such as chemistry, physics, causes the extensive concern of scientific circles.
Carbon nanotube and its reticular structure are because having special microscopic appearance and excellent physicochemical characteristics, in each field
In gather around and have broad application prospects, however, the factors such as preparation condition is cumbersome, and cost of material is higher but limit carbon nanomaterial
Development.China applies for a patent (application number 200510017038.0) and reports using polyolefin as carbon source, nickel-containing catalyst and modification
Synthesizing carbon nanotubes under montmorillonite, molecular sieve promoter effect, but modified montmorillonoid used in this method, molecular sieve price are higher,
In addition, causing pollution to environment using hydrofluoric acid removal montmorillonite and molecular sieve purification carbon nanotube.In the present invention, nanoscale
The addition of carbon black can not only improve carbon nanotube yield, its own is alternatively arranged as the formation raw material of carbon nanotube.It is bis- using Co-Mo
Metallic catalyst, the characteristics of making prepared carbon nanotube possess small diameter tube, narrow ditribution and superelevation draw ratio.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of carbon nanotube.The present invention is using polyolefin and recycling polyolefin
For carbon source, load type double-metal Co-Mo is catalyst, and using carbon black as additive, catalytic pyrolysis prepares carbon and receives under an inert atmosphere
Mitron makes waste plastic be recycled, and alleviates " white pollution ".
The present invention prepares the step of carbon nanotube and condition is as follows:
(a) preparation of Co-Mo/MgO catalyst
It is fully ground in mortar after being crushed cobalt nitrate, ammonium molybdate, magnesium nitrate with high speed disintegrator, is in molar ratio 1-
It is dissolved, is sufficiently stirred, standing is put afterwards for 24 hours with appropriate polyethylene glycol 200 after 10 parts of cobalts, 0.05-2.5 parts of molybdenums and 1-10 parts of magnesium mixing
Enter and calcine 1h in 650 DEG C of Muffle furnaces, collect product, be cooled to room temperature, with mortar grinder at about 1 μm of partial size of powder to get negative
Load type bimetallic Co-Mo/MgO catalyst.
(b) polyolefin-carbon black-catalyst mixture preparation
By the catalyst of polyolefin, carbon black and step (a) preparation in 160-200 DEG C in torque rheometer, 50 turns of revolving speed/
Polyolefin blend was made in melting mixing 5-10 minutes second；Wherein press quality ratio of components, polyolefin 60-98%, carbon black 1-
20%, catalyst 1-20%.
(c) preparation and purification of carbon nanotube
Polyolefin blend prepared by step (b) is put into quartz ampoule, the nitrogen that logical 15min flow is 50mL/min is set
It changes after inner air tube for quartz ampoule to be put into and have warmed up to 800-1000 DEG C of tube type resistance furnace.Quartz ampoule is taken out after 10min, it is cold
But to room temperature, stop logical nitrogen, collecting black carbon product is carbon nanotube product.
Resulting carbon nano tube products are flowed back in HCl solution and are boiled greater than 6 hours, to remove catalyst residue,
It is washed out to pH neutrality, and 24 hours dry at 110 DEG C, the carbon nanotube purified.
With existing technical problem, the beneficial effects of the invention are as follows low as carbon source price using polyolefin or recycling polyolefin
Honest and clean, abundance, can alleviate plastics makes resource be recycled the pollution of environment；It is urged with novel dual metal cobalt and molybdenum
Agent makes the carbon nanotube synthesized have the characteristics that small diameter tube, narrow ditribution and high length-diameter ratio；Use nanoscale carbon black as adding
Add agent, it is cheap, it is easy to get, avoids polluting the environment using hydrofluoric acid purification carbon nanotube, at the same time as carbon nanometer
Pipe raw material；The mixing apparatus used is the conventional equipment of Polymer Processing, and cracker is that general small-molecule chemical gas phase fills
It sets.With using equipment simple, easy to operate, at low cost, the high feature of carbon nanotube yield.Advantage in summary, the present invention
The method cost for preparing carbon nano-tube material have the characteristics that itself than other methods, relatively other polymeric carbon sources synthesize carbon
Nanotube has unique advantage.
Detailed description of the invention
Fig. 1 is the electron scanning micrograph for showing the carbon nanotube that example 1 is prepared.
Fig. 2 is the transmission electron microscope photo for showing the carbon nanotube that example 1 is prepared.
Fig. 3 is the purification carbon nanotube heat stability testing analysis for showing example 1 and preparing.
Fig. 4 is to show example 1 (a), example 2 (b) and example 3 (c) preparation gained carbon product XRD spectra.
Fig. 5 is the XRD spectra for showing the catalyst of different mol ratio.
Fig. 6 is the Raman spectrogram for showing example 1 (a), carbon product prepared by example 2 (b).
Specific embodiment
Embodiment 1
Co-Mo/MgO catalyst is prepared by combustion method.With high speed disintegrator respectively by cobalt nitrate, ammonium molybdate, magnesium nitrate
It is fully ground in mortar after crushing, is dissolved by after the molar ratio mixing of 1:0.5:1 with appropriate polyethylene glycol 200, sufficiently stirred
It mixes, standing, which is put into afterwards for 24 hours in 650 DEG C of Muffle furnaces, calcines 1h, collects product, is cooled to room temperature, with mortar grinder at about 1 μm of partial size
Powder, obtain load type double-metal Co-Mo/MgO catalyst.
Turn by weight being 150 DEG C in temperature for 86% polyethylene, 7% Co-Mo-Mg catalyst and 7% carbon black
10min is uniformly mixed in the torque rheometer that speed is 50rpm, obtains polyethylene mixture.
Above-mentioned polymer 5g is taken to be put into quartz ampoule, after leading to the nitrogen displacement inner air tube that 15min flow is 50mL/min
Quartz ampoule is put into and is had warmed up to 1000 DEG C of vertical tube type resistance furnace.Quartz ampoule is taken out after 10min, is cooled to room temperature, and is stopped
Only lead to N2, collecting black carbon product is carbon nanotube product.
Resulting carbon nano tube products are flowed back in 20% HCl solution and are boiled 6 hours, to remove catalyst residual
Object is washed out to pH neutrality, and 24 hours dry at 110 DEG C, the carbon nanotube 2.93g purified at this time.
Embodiment 2
Co-Mo/MgO catalyst is prepared by combustion method.With high speed disintegrator respectively by cobalt nitrate, ammonium molybdate, magnesium nitrate
It is fully ground in mortar after crushing, is dissolved by after the molar ratio mixing of 2:0.5:1 with appropriate polyethylene glycol 200, sufficiently stirred
It mixes, standing, which is put into afterwards for 24 hours in 650 DEG C of Muffle furnaces, calcines 1h, collects product, is cooled to room temperature, with mortar grinder at about 1 μm of partial size
Powder, obtain load type double-metal Co-Mo/MgO catalyst.
Turn by weight being 150 DEG C in temperature for 86% polyethylene, 7% Co-Mo-Mg catalyst and 7% carbon black
10min is uniformly mixed in the torque rheometer that speed is 50rpm, obtains polyethylene mixture.
Blends described above 5g is taken, with method preparation, the purification of example 1, obtains carbon nanotube 3g.
Embodiment 3
Co-Mo/MgO catalyst is prepared by combustion method.With high speed disintegrator respectively by cobalt nitrate, ammonium molybdate, magnesium nitrate
It is fully ground in mortar after crushing, is dissolved by after the molar ratio mixing of 3:0.5:1 with appropriate polyethylene glycol 200, sufficiently stirred
It mixes, standing, which is put into afterwards for 24 hours in 650 DEG C of Muffle furnaces, calcines 1h, collects product, is cooled to room temperature, with mortar grinder at about 1 μm of partial size
Powder, obtain load type double-metal Co-Mo/MgO catalyst.
Turn by weight being 150 DEG C in temperature for 86% polyethylene, 7% Co-Mo-Mg catalyst and 7% carbon black
10min is uniformly mixed in the torque rheometer that speed is 50rpm, obtains polyethylene mixture.
Blends described above 5g is taken, with method preparation, the purification of example 1, obtains carbon nanotube 2.97g.
Embodiment 4
Co-Mo/MgO catalyst is prepared by combustion method.With high speed disintegrator respectively by cobalt nitrate, ammonium molybdate, magnesium nitrate
It is fully ground in mortar after crushing, is dissolved by after the molar ratio mixing of 4:0.5:1 with appropriate polyethylene glycol 200, sufficiently stirred
It mixes, standing, which is put into afterwards for 24 hours in 650 DEG C of Muffle furnaces, calcines 1h, collects product, is cooled to room temperature, with mortar grinder at about 1 μm of partial size
Powder, obtain load type double-metal Co-Mo/MgO catalyst.
Turn by weight being 150 DEG C in temperature for 86% polyethylene, 7% Co-Mo/MgO catalyst and 7% carbon black
10min is uniformly mixed in the torque rheometer that speed is 50rpm, obtains polyethylene mixture.
Blends described above 5g is taken, with method preparation, the purification of example 1, obtains carbon nanotube 3.04g.
Embodiment 5
It is in temperature by weight by 7% Co-Mo/MgO catalyst in example 3,86% polypropylene and 7% carbon black
10min is uniformly mixed in the torque rheometer that 180 DEG C of revolving speeds are 50rpm, obtains polypropylene miser.
Blends described above 5g is taken, with method preparation, the purification of example 1, obtains carbon nanotube 2.87g.
Embodiment 6
Co-Mo/MgO catalyst is prepared by combustion method.With high speed disintegrator respectively by cobalt nitrate, ammonium molybdate, magnesium nitrate
It is fully ground in mortar after crushing, is dissolved by after the molar ratio mixing of 3:0.1:1 with appropriate polyethylene glycol 200, sufficiently stirred
It mixes, standing, which is put into afterwards for 24 hours in 650 DEG C of Muffle furnaces, calcines 1h, collects product, is cooled to room temperature, with mortar grinder at about 1 μm of partial size
Powder, obtain load type double-metal Co-Mo/MgO catalyst.
Turn by weight being 150 DEG C in temperature for 86% polypropylene, 7% Co-Mo/MgO catalyst and 7% carbon black
10min is uniformly mixed in the torque rheometer that speed is 50rpm, obtains polyethylene mixture.
Above-mentioned polymer 5g is taken to be put into quartz ampoule, after leading to the nitrogen displacement inner air tube that 15min flow is 50mL/min
Quartz ampoule is put into and is had warmed up to 800 DEG C of vertical tube type resistance furnace.Quartz ampoule is taken out after 10min, is cooled to room temperature, and is stopped
Logical N2, collecting black carbon product is carbon nanotube product.
With the Methods For Purification of example 1, carbon nanotube 1.32g is obtained.
Embodiment 7
Co-Mo/MgO catalyst is prepared by combustion method.With high speed disintegrator respectively by cobalt nitrate, ammonium molybdate, magnesium nitrate
It is fully ground in mortar after crushing, is dissolved by after the molar ratio mixing of 3:0.15:1 with appropriate polyethylene glycol 200, sufficiently stirred
It mixes, standing, which is put into afterwards for 24 hours in 650 DEG C of Muffle furnaces, calcines 1h, collects product, is cooled to room temperature, with mortar grinder at about 1 μm of partial size
Powder, obtain load type double-metal Co-Mo/MgO catalyst.
With method preparation, the purification of example 5, carbon nanotube 1.78g is obtained.
Embodiment 8
It is in temperature by weight by 7% Co-Mo/MgO catalyst in example 1,82% polyethylene and 1% carbon black
10min is uniformly mixed in the torque rheometer that 180 DEG C of revolving speeds are 50rpm, obtains polyethylene mixture.
With method preparation, the purification of example 1, carbon nanotube 2.09g is obtained.
Embodiment 9
It is in temperature by weight by 7% Co-Mo/MgO catalyst in example 1,90% polyethylene and 3% carbon black
10min is uniformly mixed in the torque rheometer that 180 DEG C of revolving speeds are 50rpm, obtains polyethylene mixture.
With method preparation, the purification of example 1, carbon nanotube 2.34g is obtained.
Embodiment 10
It is in temperature by weight by 7% Co-Mo/MgO catalyst in example 1,88% polyethylene and 5% carbon black
10min is uniformly mixed in the torque rheometer that 180 DEG C of revolving speeds are 50rpm, obtains polyethylene mixture.
With method preparation, the purification of example 1, carbon nanotube 2.65g is obtained.
Embodiment 11
It is in temperature by weight by 7% Co-Mo/MgO catalyst in example 1,84% polyethylene and 9% carbon black
10min is uniformly mixed in the torque rheometer that 180 DEG C of revolving speeds are 50rpm, obtains polyethylene mixture.
With method preparation, the purification of example 1, carbon nanotube 3.02g is obtained.
Embodiment 12
It is in temperature by weight by 1% Co-Mo/MgO catalyst in example 1,94% polyethylene and 5% carbon black
10min is uniformly mixed in the torque rheometer that 180 DEG C of revolving speeds are 50rpm, obtains polyethylene mixture.
With method preparation, the purification of example 1, carbon nanotube 1.52g is obtained.
Embodiment 13
It is in temperature by weight by 3% Co-Mo/MgO catalyst in example 1,92% polyethylene and 5% carbon black
10min is uniformly mixed in the torque rheometer that 180 DEG C of revolving speeds are 50rpm, obtains polyethylene mixture.
With method preparation, the purification of example 1, carbon nanotube 2.19g is obtained.
Embodiment 14
It is in temperature by weight by 5% Co-Mo/MgO catalyst in example 1,90% polyethylene and 5% carbon black
10min is uniformly mixed in the torque rheometer that 180 DEG C of revolving speeds are 50rpm, obtains polyethylene mixture.
With method preparation, the purification of example 1, carbon nanotube 2.51g is obtained.
Embodiment 15
It is in temperature by weight by 9% Co-Mo/MgO catalyst in example 1,86% polyethylene and 5% carbon black
10min is uniformly mixed in the torque rheometer that 180 DEG C of revolving speeds are 50rpm, obtains polyethylene mixture.
With method preparation, the purification of example 1, carbon nanotube 2.84g is obtained.
Embodiment 16
By weight by 7% Co-Mo/MgO catalyst in example 3,86% polystyrene and 7% carbon black in temperature
It is uniformly to mix 10min in the torque rheometer of 50rpm for 190 DEG C of revolving speeds, obtains polystyrene blends.
Blends described above 5g is taken, with method preparation, the purification of example 1, obtains carbon nanotube 3.25g.
Embodiment 17
By weight by 7% Co-Mo/MgO catalyst in example 1,86% recycle polyethylene and 7% carbon black in temperature
Degree is that 150 DEG C of revolving speeds are that 10min is uniformly mixed in the torque rheometer of 50rpm, obtains recycle polyethylene mixture.
Blends described above 5g is taken, with method preparation, the purification of example 1, obtains carbon nanotube 3.35g.
Embodiment 18
By weight by 7% Co-Mo/MgO catalyst in example 2,86% recycle polyethylene and 7% carbon black in temperature
Degree is that 150 DEG C of revolving speeds are that 10min is uniformly mixed in the torque rheometer of 50rpm, obtains recycle polyethylene mixture.
Blends described above 5g is taken, with method preparation, the purification of example 1, obtains carbon nanotube 3.16g.
Embodiment 19
By weight by 7% Co-Mo/MgO catalyst in example 3,86% recycle polyethylene and 7% carbon black in temperature
Degree is that 150 DEG C of revolving speeds are that 10min is uniformly mixed in the torque rheometer of 50rpm, obtains recycle polyethylene mixture.
Blends described above 5g is taken, with method preparation, the purification of example 1, obtains carbon nanotube 3.49g.
Claims (6)
1. a kind of preparation method of carbon nanotube is characterized in that step and condition are as follows:
(1) preparation of Co-Mo/MgO catalyst
Cobalt nitrate, ammonium molybdate, magnesium nitrate are sufficiently mixed with physical mechanical method, are in molar ratio 1-10 parts of cobalts, 0.05-2.5
It is dissolved, is sufficiently stirred, standing is put into afterwards for 24 hours in Muffle furnace with appropriate polyethylene glycol 200 after part molybdenum and 1-10 parts of magnesium mixing
500-800 DEG C of calcining 1h collects product, is cooled to room temperature, double to get support type at about 1 μm of partial size of powder with mortar grinder
Metal Co-Mo/MgO catalyst.
(2) polyolefin-carbon black-catalyst mixture preparation
The catalyst of polyolefin, carbon black and step (1) preparation is utilized into twin-screw extrusion or torque rheometer at 160-200 DEG C
Polyolefin blend is made in melt blending；Wherein press quality ratio of components, polyolefin 60-98%, carbon black 1-20%, catalyst
For 1-20%.
(3) preparation and purification of carbon nanotube
Polyolefin blends prepared by step (2) are put into quartz ampoule, are put quartz ampoule using after nitrogen displacement inner air tube
Enter and has warmed up to 800-1000 DEG C of tube type resistance furnace.Quartz ampoule is taken out after being cooled to room temperature, and is stopped logical nitrogen, is collected black
Color carbon product is carbon nanotube product.
Resulting carbon nano tube products are flowed back in HCl solution and are boiled greater than 6 hours, to remove catalyst residue, then
Washing is neutral to pH, and 24 hours dry at 110 DEG C, the carbon nanotube purified.
2. a kind of preparation method of carbon nanotube according to claim 1, which is characterized in that polyolefin used is various boards
Number polyethylene, polypropylene, polystyrene or its reclaimed materials.
3. a kind of preparation method of carbon nanotube according to claim 1, which is characterized in that MgO used can use stone
Ink, quartz, silicon, silicon carbide, silica, aluminium oxide, aluminosilicate (zeolite), calcium carbonate etc. replace.
4. a kind of preparation method of carbon nanotube according to claim 1, which is characterized in that carbon black used is micron
And Nano grade, it can be colour carbon black, superconductive carbon black, acetylene carbon black, rubber black, black carbon special etc..
5. a kind of preparation method of carbon nanotube according to claim 1, which is characterized in that the catalyst is micron
Or Nano grade, Co can be oxidation state and metallic state, catalyst can pass through high-temperature calcination or the lower system of inert gas shielding cracking
?.
6. a kind of preparation method of carbon nanotube according to claim 1, which is characterized in that the blend blending side
Method is that melt blending or physical mechanical are blended, and blending temperature is when wherein polyolefin is the polyethylene kind of polyethylene kind and recycling
150 DEG C, PP type and the blending temperature for recycling PP type are 180 DEG C, and polystyrene type is total to recycling polystyrene type
Mixed temperature is 190 DEG C.
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| CN114455967A (en) * | 2022-01-27 | 2022-05-10 | 西安建筑科技大学 | Low-carbon refractory material additive, preparation method and application |
| CN114515578A (en) * | 2021-12-31 | 2022-05-20 | 佛山市格瑞芬新能源有限公司 | Catalyst for preparing carbon nano tube and preparation method and application thereof |
| CN114572967A (en) * | 2022-04-07 | 2022-06-03 | 暨南大学 | System for solid polyolefin second-order firing carbon nano tube |
| CN114634174A (en) * | 2020-12-16 | 2022-06-17 | 东北林业大学 | Method for synthesizing carbon nano tube by using starch or cellulose biomass as carbon source |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114634174A (en) * | 2020-12-16 | 2022-06-17 | 东北林业大学 | Method for synthesizing carbon nano tube by using starch or cellulose biomass as carbon source |
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| CN114572967B (en) * | 2022-04-07 | 2023-10-20 | 暨南大学 | System for second order firing of carbon nano tube by solid polyolefin |
| CN114855305A (en) * | 2022-04-25 | 2022-08-05 | 延边大学 | Preparation method of carbon nanofiber material |
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